High flavor load particle and method of preparing same

ABSTRACT

The present invention relates to high flavor load particles and to methods of preparing same. The invention also relates to methods of using such particles to flavor tobacco products, including cigarettes and other conventional smoking articles.

This application claims priority from U.S. Provisional Appln. No. 60/565,522, filed Apr. 27, 2004, and U.S. Provisional Appln No. 60/592,244 and EP 04103681.5, filed Jul. 30, 2004, the entire contents of which are incorporated herein by reference.

FIELD OF THE INVENTION

The present invention relates to high flavor load particles and to methods of preparing same. The invention also relates to methods of using such particles to flavor tobacco products, including cigarettes and other conventional smoking articles.

BACKGROUND OF THE INVENTION

Flavoring agents that are added to tobacco products, including cigarettes, are typically subjected to combustion as the tobacco burns. The combustion of such agents can result in the formation of harmful substances, at least some of which are considered carcinogenic.

In a typical cigarette manufacturing process, flavoring agents are first added to the tobacco leaf by spraying dilute solutions of the flavoring agents directly onto the cut leaf, or by applying liquid or dry flavoring agents during the reconstituted sheeting process. The amount of dry or liquid flavoring agent applied directly to reconstituted sheet filler or directly to the leaf can be as high as 4-5% of the cigarette filler weight. The reconstituted sheeting consists of sheeted stem, seeds, and/or roots from the tobacco plant; waste dust resulting from cigarette manufacture and collected from the production-plant floor can also be included. These waste products, combined with cellulose pulp, are sheeted in a manner similar to the traditional paper making process and are shredded in the same dimensions as the quality tobacco cut leaf and blended into the tobacco filler to extend and cut the cost of cigarette manufacture. Reconstituted sheet can comprise 10-20% of the cigarette rod weight.

Liquid flavoring agents are also sometimes sprayed onto the filter cellulose of cigarettes and are delivered with the steam that is entrained through the cigarette rod. Only small amounts of the flavoring agents can be applied, otherwise they will interfere with the smoke taste and perception in the mouth. Spray-dried flavoring agents have been attempted but it has been found that they are susceptible to migration through the filter, with the potential to be inhaled into the lungs. Further, spray-dried flavoring agents are susceptible to migration from the cigarette rod into the packaging.

The present invention relates to an improved approach to delivering flavor to tobacco products, such as cigarettes and other conventional smoking articles (e.g., cigars and cigarillos). The invention provides, for example, a “safer” traditional cigarette that results in reduced harm to the lungs of the smoker while imparting enhanced flavor impact.

In accordance with the invention, spheronized particles embedded with flavoring agent(s) are positioned in the tobacco product, such as a cigarette, such that they do not undergo combustion, thereby avoiding production of harmful pyrolysis products. The instant particles can be positioned in the filter cavity of a traditional cigarette between the tobacco rod and the cellulose filter. The particles are of sufficient size and durability that they do not become dislodged.

SUMMARY OF THE INVENTION

The present invention relates to high flavor load spherical particles (advantageously, symmetrically spherical) comprising a matrix material (e.g., a porous matrix material) that can absorb many times its weight in fluid, and at least one flavoring agent and/or excipient and/or aerosolizing agent. The instant particles make it possible for the tobacco industry to provide to the public a “safer” traditional cigarette that delivers flavors and/or excipients in a non-pyrolized form.

The invention includes the spherical particles, as well as intermediates in the process of producing such particles, including a semi-dry dough or paste resulting from mixing of the matrix material with the flavoring agent and/or excipient.

The invention also includes a method of preparing the spherical particles, for example, a method in which a low pressure extrudate is converted into spherical granules through a spheronization process.

The invention further includes a cigarette-type smoking article comprising the particles of the invention. Release of flavor from the particles is obtained through non-pyrolysis steam entrainment.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a flow chart of the process of making the particles of the invention.

FIG. 2 is a longitudinal cross section of an exemplary embodiment of the invention.

DETAILED DESCRIPTION OF THE INVENTION

The present invention relates to particles (e.g., spherical particles) comprising a matrix (e.g., a porous matrix) and at least one material (e.g., a flavoring agent) embedded (“loaded”) therein. The particles are suitable for use in the tobacco industry, particularly, in the production of cigarettes and other conventional smoking articles (e.g., cigars, cigarillos, etc).

The matrix of the spherical particles of the invention can comprise cellulose, modified cellulose, or other carbohydrate (such as natural or synthetic gum, pectin or starch), natural or synthetic protein (for example, gelatin), or other material (e.g., low dextrose equivalent carbohydrate (e.g., corn, rice or hydrolyzed cereal (grain) solids)) (or mixtures thereof) that, preferably, can absorb many times its weight in fluid (advantageously, about two to five times). Preferably, the matrix is cellulose as it has good particle integrity, it is insoluble in water, it is compatible with tobacco regulatory practice and appears on the tobacco 599 list. More preferably, the matrix is microcrystalline cellulose.

Typically, the matrix is loaded with a flavoring agent (e.g., vanillin, cocoa, licorice, menthol or other synthetic or natural material within the FEMA GRAS list permissible within tobacco additive law and that appears on the tobacco 599 list) and/or a substance that promotes aerosolization, such as glycerin, or other polyol (e.g., propylene glycol or triethylene glycol). The amount of absorbed aerosolization promoting agent can be 1% to 40%, preferably 10%-35%, more preferably 28%-30% w/w of the particle. The particles can also comprise one or more additives, such as activated carbon (charcoal) (shown in tobacco filter design literature to filter smoke compounds), diatomaceous earth (shown to absorb fat and oil based compounds such as botanical tar), silica or silicates (shown to absorb water and oil based compounds), and/or α-, β-, and/or γ-cyclodextrins (shown to trap and encapsulate hydrophobic compounds).

The particles of the invention can further comprise a thin coating that protects the loaded matrix during storage. For example, the coating can range from about 2.5% of the weight of the particle to about 15% of the weight of the particle. One such coating comprises, for example, hydroxypropyl methyl cellulose or carboxymethyl cellulose. The particles of the invention can also comprise a coating (e.g., a polymer coating, for example, a Food Grade edible polymer permissible within the tobacco regulation (i.e., the tobacco 599 list) that serves to sustain release of the flavoring agent and/or other material embedded in the matrix. Coatings of about 2.5% to about 15% of particle weight can be used.

The particles of the invention are preferably symmetrical and from about 0.3 millimeters (mm) to about 10 mm in diameter, more preferably about 0.3 mm to about 1.5 mm and still more preferably about 0.7 mm to about 1.2 mm in diameter. (A US sieve size 14 should accommodate about 95% of 0.7 mm particles.)

Particles of the invention can be prepared using, for example, a process that includes the production of a low-pressure extrudate that is converted into spherical granules through a spheronization process. More specifically, particles can be prepared by the following process:

i) Mixing dry matrix and material to be loaded (e.g., liquid flavoring agent or solution (advantageously aqueous, however, hydrophobic solutions can be used) of flavoring agent and/or aerosolizing agent) in, for example, a planetary mixer—advantageously, the material to be loaded does not exceed 75% W/W of the resulting composition and the matrix is not less than 25% W/W of the resulting composition. The composition is mixed until a malleable dough-like paste is formed and all liquid has been uniformly absorbed onto the matrix. For purposes of clarity, an example of a working formula is as follows: Glycerin 2,4870 56-81-5 2525 182,132 Diluent Ashland Chemical Inc. Propylene Glycol 2,4870 57-55-6 2940 184,1666 Diluent Univar USA Inc Micro Crystalline Cellulose 29,0000 65996-61-4 N/A 186,1673 Carrier FMC Corp. Water 50,2900 Diatomaceous Earth (Silica) 4,1400 91053-39-3 N/A Carrier Seegott Inc Charcoal, Activated Untreated 8,2900 64365-11-3 N/A Carrier American Norit Co. Total 100,0000

ii) Before the dough-like paste resulting from step (i) is subjected to extrusion, a die press channel for the extruder is selected based on the desired size of the finished spheres (typically, the diameter of the die press channel ranges from 0.1 mm-10.0 mm, 0.7 mm being preferred). The size selected defines the cross-section of the extrudate rods produced. Other parameters to be determined include the temperature of the cooling jacket shaft around the extruder screw, the roller speed and the gear speed, and the pressure at the dieface (optimum conditions will be depend, for example, on the extruder used and material extruded).

iii) The dough-like paste resulting from step (i) can then be introduced (manually or automatically) into the extruder selected of step (ii) (which is preferably a low-pressure extruder in which the temperatures at the dieface surface are lower, which minimizes volatile flavoring agents absorbed in the dough from flashing off, as would be the case in a high pressure extruder. Introduction (feed) of the dough-like paste into the input shaft can be performed in batches (Batch Mode) or continuously (Continuous Mode), or a Batch-Continuous method can be used. Feed and output rates are determined by the roller, which is a shaft within the extruder that-pulls the dough into the screws so that the screws can push the dough through the dieface. The extruder can be single, twin or axial twin screw and can be designed for gravity feed and low pressure extrusion.

iv) The extrudate resulting from step (iii) has a rod shape and the rods can be collected and transferred (manually or by machine) directly into the spheronizing unit. The rods can be gravity fed into the spheronization chamber and are allowed to fall onto the spinning friction plate. The spinning rate of the friction plate is, advantageously, about 80 RPM. The friction plate propels the particles against the jacketed walls of the unit by centrifugal force, whereby the rods are broken into smaller segments. Centrifugal and gravitational forces create a mechanically fluidized ring of these smaller segments or particles. Collisions with the wall, the baffled friction plate and other particles, result in plastic deformation of each granule and, after a resonance time of about 1.5-3 minutes, they become semi-moist and adopt a uniform and spherical form.

v) The semi-moist uniform spheres resulting from step (iv) can be discharged into a fluid bed dryer and dried to the desired moisture content, which typically ranges from 2-8%. The spheres can also be thin film coated if desired. (See also FIG. 1 and Example 1.)

Extruders suitable for use in the preset method include those made by, for example, LCI,4409-C Chesapeake Drive, P.O. Box 16348, Charlotte, N.C. 28297, Hosokawa Bepex, 333 N.E. Taft Street, Minneapolis, Minn. 55413, and Caleva Process Solutions Ltd, Butts Pond Industrial Estate, Sturminster Newton, Dorset DT 101AZUK. Spheronizing units suitable for use include those made by, for example, LCI, Hosokawa Bepex, and Caleva.

Particles prepared using the above-described method are substantially uniform in size and weight and typically larger (for example, about 60-80 mesh) than particles resulting from traditional spray-drying processes (100-120 mesh). These characteristics have advantages when machine filling is used in the preparation of the ultimate smoking article. The ability to control particle size makes it possible to deposit an exact number of particles, uniform in size and shape. A single particle having a large diameter can also be used (for example, a single pellet large enough (about 5 mm) to occupy a space in a traditional cigarette between the filter and the tobacco). The smooth surface of particles produced by the spheronization process allows any coating to be uniformly applied.

The mixing and extrusion steps of the process of the invention, in contrast to the traditional spray-drying process, result in the production of particles that are also uniform with respect to concentration of the material (e.g., flavoring agent) embedded within the matrix.

The particle preparation methods described herein result in high yields, losses of other than moisture are minimal. By way of example, recoveries of about 98% of cellulose and non-water soluble components (such as, for example, propylene glycol, glycerin, botanical matter, and FEMA (Flavor Extract Manufacturers Association) GRAS (Generally Accepted As Safe) chemicals) can be obtained.

The present method is non-dusting for production application in comparison with traditional methods. Even a layman with a visual check can easily determine a reduced dusting, because a reduced dusting results when the product of the invention is shaken or moved, in comparison with that of the traditional method.

The particles of the invention can be present, for example, in a traditional cigarette between the tobacco rod and the cellulose filter. The number of particles used can vary, for example, with the particle size. Typically, the particles occupy about 3 mm to about 10 mm of the overall length of the cigarette. The particles can be loaded into the cigarette mechanically.

Depicted in FIG. 2 is a smokable article, e.g., a cigarette, that embodies the instant invention. The cigarette, generally indicated 10, comprises a cylindrical rod 12 containing smokable material 14 (e.g., tobacco) wrapped in at least one layer of a circumscribing outer wrapping material 16 (e.g., paper), and a filter element 18. Positioned between the smokable material 14 and the filter element 18 in rod 12 are particles 20 embedded with at least one flavoring agent and at least one agent that promotes aerosolization in accordance with a preferred embodiment of the present invention.

According to the invention, the flavoring agent(s) is/are released from the particles by a indirect heating method within a filter system wherein steam from the burning tobacco stick is pulled through the filter. The moisture causes the particle matrix (e.g., cellulose) to swell. The flavoring agent is then displaced from the particle and mixes with the moist steam and is entrained through the filter system. As the flavoring agent(s) are not combusted, pyrolysis products, such as tar, hydrocarbons and nitrosamines, are not produced.

The primary function of the instant particles is to serve as a delivery for non-combusted flavoring agents within, for example, a cigarette filter system. However, the particles, particularly particles that include additives such as charcoal, diatomaceous earth, silica, silicates and/or cyclodextrins, can act as a filtration device for harmful compounds contained in, for example, cigarette smoke.

Certain aspects of the present invention are described in greater detail in the non-limiting Examples that follow.

EXAMPLE 1

Particles of the invention can be prepared using the process that follows:

-   1. A hydrophilic flavor agent is applied to a dry matrix comprising     of microcrystalline cellulose at a 50/50 w/w ratio to form a     dough-like paste. -   2. The dough resulting from step 1 is fed, automatically or     manually, into a low-pressure extruder and extruded through a die     face grid screen with a preferred grid size of 0.5 mm-1.0 mm, which     defines the cross section of the particle rod. The extruder can be     single or twin screw or axial twin screw, which is designed for     gravity feed and low pressure extrusion or jacketed cooling of the     extruder shaft. The unit has the capacity to extrude rods down to     0.3 mm with rod integrity. -   3. The rods resulting from step 2 are delivered, manually or by     machine, to a spheronizing unit. The spheronizer comprises a     vertical cylinder with a discharge shaft or port, a circular multi     baffled “friction” plate (e.g., 1 mm-5 mm disk) and a variable speed     drive train that rotates the plate. -   4. The rods are fed into the spinning friction plate chamber at 80     RPM for 1.5-3 minutes. The friction plate propels the rods against     the inside wall of the unit by centrifugal force and, as a result,     the rods are broken into smaller segments. Centrifugal and     gravitational forces create a mechanically fluidized ring of     particles. Collisions with the wall, the baffled friction plate and     other particles, results in plastic deformation of each granule,     which gives rise to the creation of a uniform spherical shape. The     time the particles spend in this unit is referred to as the     “resonance time” or the spheronization time, and it equals the time     it takes to form spheres from the total volume of extrudate rods. -   5. The semi-moist spheres resulting from step 4 are then dried in a     belt fluid bed system until the desired moisture content is     achieved. -   6. The semi-moist spheres are finally thin film coated.

EXAMPLE 2

Described below is a process to deliver flavor post rod filler in a cavity beneath a cigarette filter. Theoretically, cellulose will swell, discharging flavor into entrained air flow.

Materials:

-   i) Tobacco Type flavor (composed of FEMA GRAS materials, the flavor     can be a mix consisting of the following at the limits not to exceed     the described maximum all described in percentage of the overall     flavoring preparation: Acetanisole <1, Acetic Acid <100,     Acetophenone <10, Ammonium Hydroxide <100, Benzaldehyde <1, Benzoin     Resinoid <50, Benzyl Alcohol <100, Bergamot Oil <10, Bornyl Acetate     <1, Butyric Acid <1, Cardamon Seed Oil <1, Carob Bean Extract <100,     Celery Seed Oil <1, Chamomile Flower Oil Hungarian <5, Chamomile     Flower Oil Roman <5, Cinnamic Aldehyde <50, Cinnamic Alcohol <1,     Citral <1, Citric Acid <1, D,L Citronellal <1, Clary Sage Oil <5,     Cocoa and Cocoa extracts <100, Coffee Extract <50, Cognac oil Green     <1, Coriander Oil <5, Davana Oil <1, Delta Decalactone <1, Gamma     Decalactone <1, Decanoic Acid <1, Diacetyl <1, Diammonium Phosphate     <100, 2,3-Dimethyl Pyrazine <1, Dill Oil <1, 2,5 Dimethyl Pyrazine     <1, Ethyl Acetate <50, Ethyl Hexanoate <50, Ethyl Iso Valerate <1,     Ethyl Lactate <1, Ethyl Maltol <1, Ethyl Octanoate <1, Ethyl     Phenylacetate <1, Ethyl Propionate <5, Ethyl Vanillin <10,     5-Ethyl-3-Hydroxy-4-Methyl-2(5H)-Furanone <1, Fenugreek Extract <10,     Geraniol <1, Geranium Rose Oil <1, Glycerine <100, 2-Heptanone <5,     Hexanoic Acid <1, Hexyl Acetate <1,     4-(Para-Hydroxyphenyl)-2-butanone <1, Immortelle Extract <1, Alpha     Ionone <1, Isoamyl Acetate <1, Isoamyl Butyrate <1, Isoamyl Formate     <1, Isoamyl Hexanoate <1, Isoamyl Isovalerate <1, Isoamyl Phenyl     Acetate <1, Iso Butric Acid <5, Isovaleric Acid <1, Licorice Extract     <100, Lime Oil <5, Linalool <1, Lovage Extract <100, Maltol <50,     Mate Absolute <10, L-Menthol <100, 2-Mercapto Methyl Pyrazine <1,     Para-Methoxy Benzaldehyde <10, Methyl Isovalerate <1,     4-Methoxyacetphenone <5, 3-Methylbutyraldehyde <50, 2-Methyl Butyric     Acid <1, Methyl Cyclopentenelone <50, Mimosa Absolute <1, Mountain     Maple Extract <100, Gamma Nonalactone <1, Oakmoss Absolute <10,     Gamma Octalactone <1, Opoponox Oil <5, Orange Oil <50, Orris Root     Extract <50, Peppermint Oil <100, Phenylethyl Alcohol <1,     Phenylethyl Phenylacetate <50, Phenyl Acetic Acid <5, Heliotropine     <5, Vanitrope <1, Propylene Glycol <100, Rhodinol <1, Rose Oil Otto     Bulgarian <1, Rum <100, Non-Alcoholic Rum <1, Sandalwood Oil <5,     Scarolide <10, Styrax Resin <1, High Fructose Corn Syrup 42% Solids     <100, Invert Sugar Syrup <100, Sucrose <100, Tangerine Oil <5, Alpha     Terpineol <5, 2,3,5,6 Tetramethylpyrazine <1, Para Tolyl Aldehyde     <1, 4-(2,6,6-Trimethyl Cyclohex-1-enyl) but-2-en-one <1,     2,3,5-Trimethylpyrazine <1, Gamma Undecalactone <1, Valerian Root     Extract <100, Vanilla Bean Extract <10, Vanillin <100) (Chr. Hansen)     (4.55% W/W wet basis, 9.1% load dry basis). -   ii) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (45.45%     W/W wet basis, 90.9% load dry basis). -   iii) Deionized water (50.00% W/W wet basis).

The process comprises the following steps:

-   A) add Avicel and flavor to a planetary mixer; -   B) blend until visually uniform; -   C) add deionized water while mixing until visually uniform; -   D) extrude in a coaxial jacketed dome extruder to the     specifications: 0.7 mm stainless steel dieface at an auger speed of     45 rpm inserting 10 shims at the dome contact point; -   E) collect damp extrudate rods and deposit into a     Maumerizing/Spheronizing centrifugal unit—parameters are: 2.0 mm     disk plate at a speed of 1200 rpm for a resonance time of 3 minutes;     and -   F) dry in Glatt Fluid Bed Dryer (<90° C.) target moisture is <20%.

The resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.10 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade. The cigarette can be lit in a conventional manner and flavor delivery evaluated.

EXAMPLE 3

Described below is a process to deliver higher flavor load post rod filler in a cavity beneath the filter. As above, the cellulose will swell, discharging flavor into entrained air flow.

Materials:

-   i) Tobacco Type (composed of FEMA GRAS materials, the flavor can be     a mix consisting of the following at the limits not to exceed the     described maximum all described in percentage of the overall     flavoring preparation: Acetanisole <0.5, Acetic Acid <100,     Acetophenone <2.5, Ammonium Hydroxide <100, Benzaldehyde <0.5,     Benzoin Resinoid <25, Benzyl Alcohol <100, Bergamot Oil <0.5, Bornyl     Acetate <0.5, Butyric Acid <0.5, Cardamon Seed Oil <0.5, Carob Bean     Extract <100, Celery Seed Oil <0.5, Chamomile Flower Oil Hungarian     <2.5, Chamomile Flower Oil Roman <2.5, Cinnamic Aldehyde <25,     Cinnamic Alcohol <0.5, Citral <0.5, Citric Acid <0.5, D,L     Citronellal <0.5, Clary Sage Oil <2.5, Cocoa and Cocoa extracts     <100, Coffee Extract <25, Cognac oil Green <0.5, Coriander Oil <2.5,     Davana Oil <0.5, Delta Decalactone <0.5, Gamma Decalactone <0.5,     Decanoic Acid <0.5, Diacetyl <0.5, Diammonium Phosphate <100,     2,3-Dimethyl Pyrazine <0.5, Dill Oil <0.5, 2,5 Dimethyl Pyrazine     <0.5, Ethyl Acetate <25, Ethyl Hexanoate <25, Ethyl Iso Valerate     <0.5, Ethyl Lactate <0.5, Ethyl Maltol <0.5, Ethyl Octanoate <0.5,     Ethyl Phenylacetate <0.5, Ethyl Propionate <2.5, Ethyl Vanillin <5,     5-Ethyl-3-Hydroxy-4-Methyl-2(5H)-Furanone <0.5, Fenugreek Extract     <5, Geraniol <0.5, Geranium Rose Oil <0.5, Glycerine <100,     2-Heptanone <2.5, Hexanoic Acid <0.5, Hexyl Acetate <0.5,     4-(Para-Hydroxyphenyl)-2-butanone <0.5, Immortelle Extract <0.5,     Alpha Ionone <0.5, Isoamyl Acetate <0.5, Isoamyl Butyrate <0.5,     Isoamyl Formate <0.5, Isoamyl Hexanoate <0.5, Isoamyl Isovalerate     <0.5, Isoamyl Phenyl Acetate <0.5, Iso Butric Acid <2.5, Isovaleric     Acid <0.5, Licorice Extract <100, Lime Oil <2.5, Linalool <0.5,     Lovage Extract <50, Maltol <25, Mate Absolute <2.5, L-Menthol <100,     2-Mercapto Methyl Pyrazine <0.5, Para-Methoxy Benzaldehyde <5,     Methyl Isovalerate <1, 4-Methoxyacetphenone <2.5,     3-Methylbutyraldehyde <25, 2-Methyl Butyric Acid <0.5, Methyl     Cyclopentenelone <25, Mimosa Absolute <0.5, Mountain Maple Extract     <100, Gamma Nonalactone <0.5, Oakmoss Absolute <2.5, Gamma     Octalactone <0.5, Opoponox Oil <2.5, Orange Oil <25, Orris Root     Extract <25, Peppermint Oil <100, Phenylethyl Alcohol <0.5,     Phenylethyl Phenylacetate <25, Phenyl Acetic Acid <2.5, Heliotropine     <2.5 Vanitrope <0.5, Propylene Glycol <100, Rhodinol <0.5, Rose Oil     Otto Bulgarian <0.5, Rum <100, Non-Alcoholic Rum <0.5, Sandalwood     Oil <2.5, Scarolide <5, Styrax Resin <0.5, High Fructose Corn Syrup     42% Solids <100, Invert Sugar Syrup <100, Sucrose <100, Tangerine     Oil <2.5, Alpha Terpineol <2.5, 2,3,5,6 Tetramethylpyrazine <0.5,     Para Tolyl Aldehyde <0.5, 4-( 2,6,6′-Trimethyl Cyclohex-1-enyl)     but-2-en-one <0.5, 2,3,5-Trimethylpyrazine <0.5, Gamma Undecalactone     <0.5, Valerian Root Extract <100, Vanilla Bean Extract <5, Vanillin     <50) (Chr. Hansen) (9.10% W/W wet basis, 20.02% load dry-basis). -   ii) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (45.55%     W/W wet basis, 79.78% load dry basis). -   iii) Deionized water (45.45% W/W wet basis)

The process comprises the same steps set forth above in Example 2. The resulting spheres can be introduced into a cigarette rod in the manner described in Example 2 and flavor delivery evaluated.

EXAMPLE 4

Described below is a process to deliver ultra high flavor load post rod filler in a cavity beneath the filter. Again, cellulose will swell, discharging flavor into entrained air flow.

Materials:

-   i) Tobacco Type flavor (composed of FEMA GRAS materials, the flavor     can be a mix consisting of the following at the limits not to exceed     the described maximum all described in percentage of the overall     flavoring preparation: Acetanisole <0.25 Acetic Acid <100,     Acetophenone <2.5, Ammonium Hydroxide <100, Benzaldehyde <0.25,     Benzoin Resinoid <12.5, Benzyl Alcohol <100, Bergamot Oil <2.5,     Bornyl Acetate <0.25 Butyric Acid <0.25, Cardamon Seed Oil <0.25,     Carob Bean Extract <100, Celery Seed Oil <0.25, Chamomile Flower Oil     Hungarian <1.25, Chamomile Flower Oil Roman <1.25, Cinnamic Aldehyde     <12.5, Cinnamic Alcohol <0.25, Citral <0.25, Citric Acid <0.25, D,L     Citronellal <0.25, Clary Sage Oil <0.25, Cocoa and Cocoa extracts     <100, Coffee Extract <12.5, Cognac oil Green <0.25, Coriander Oil     <1.25, Davana Oil <0.25, Delta Decalactone <0.25, Gamma Decalactone     <0.25, Decanoic Acid <0.25, Diacetyl <0.25, Diammonium Phosphate     <100, 2,3-Dimethyl Pyrazine <0.25, Dill Oil <0.25, 2,5 Dimethyl     Pyrazine <0.25, Ethyl Acetate <12.5, Ethyl Hexanoate <12.5, Ethyl     Iso Valerate <0.25, Ethyl Lactate <0.25, Ethyl Maltol <0.25, Ethyl     Octanoate <0.25, Ethyl Phenylacetate <0.25, Ethyl Propionate <1.25,     Ethyl Vanillin <2.5, 5-Ethyl-3-Hydroxy-4-Methyl-2(5H)-Furanone     <0.25, Fenugreek Extract <2.5, Geraniol <0.25, Geranium Rose Oil     <0.25, Glycerine <100, 2-Heptanone <1.25, Hexanoic Acid <0.25, Hexyl     Acetate <0.25, 4-(Para-Hydroxyphenyl)-2-butanone <0.25, Immortelle     Extract <0.25, Alpha Ionone <0.25, Isoamyl Acetate <0.25, Isoamyl     Butyrate <0.25, Isoamyl Formate <0.25, Isoamyl Hexanoate <0.25,     Isoamyl Isovalerate <0.25, Isoamyl Phenyl Acetate <0.25, Iso Butric     Acid <1.25, Isovaleric Acid <0.25, Licorice Extract <100, Lime Oil     <1.25, Linalool <0.25, Lovage Extract <100, Maltol <12.5, Mate     Absolute <2.5, L-Menthol <100, 2-Mercapto Methyl Pyrazine <0.25,     Para-Methoxy Benzaldehyde <2.5, Methyl Isovalerate <0.25,     4-Methoxyacetphenone <1.25, 3-Methylbutyraldehyde <12.5, 2-Methyl     Butyric Acid <0.25, Methyl Cyclopentenelone <12.5, Mimosa Absolute     <0.25, Mountain Maple Extract <100, Gamma Nonalactone <0.25, Oakmoss     Absolute <2.5, Gamma Octalactone <0.25, Opoponox Oil <1.25, Orange     Oil <12.5, Orris Root Extract <12.5, Peppermint Oil <100,     Phenylethyl Alcohol <0.25, Phenylethyl Phenylacetate <12.5, Phenyl     Acetic Acid <0.25, Heliotropine <1.25, Vanitrope <0.25, Propylene     Glycol <100, Rhodinol <0.25, Rose Oil Otto Bulgarian <0.25, Rum     <100, Non-Alcoholic Rum <0.25, Sandalwood Oil <1.25, Scarolide <2.5,     Styrax Resin <0.25, High Fructose Corn Syrup 42% Solids <100, Invert     Sugar Syrup <100, Sucrose <100, Tangerine Oil <1.25, Alpha Terpineol     <1.25, 2,3,5,6 Tetramethylpyrazine <0.25, Para Tolyl Aldehyde <0.25,     4-(2,6,6-Trimethyl Cyclohex-1-enyl) but-2-en-one <0.25,     2,3,5-Trimethylpyrazine <0.25, Gamma Undecalactone <0.25, Valerian     Root Extract <100, Vanilla Bean Extract <2.5, Vanillin <25) (Chr.     Hansen) (20.00% W/W wet basis, 40.00% load dry basis). -   ii) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (50.00%     W/W wet basis, 60.00% load dry basis). -   iii) Deionized water (30.00% W/W wet basis).

The process comprises the same steps used in Examples 2 and 3. The resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.07 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade. The cigarette can be lit in a conventional manner and flavor delivery evaluated.

In this procedure, flavor seemed to leach out of spheres, and this flavor load may be too high and should be optimized.

EXAMPLE 5

Described below is a further process to deliver ultra high flavor load post rod filler in a cavity beneath the filter. This trial represents optimized level of flavor embedded. As indicated above, cellulose will swell, discharging flavor into entrained air flow.

Materials:

-   i) Tobacco Type flavor (composed of FEMA GRAS materials, the flavor     can be a mix consisting of the following at the limits not to exceed     the described maximum all described in percentage of the overall     flavoring preparation: Acetanisole <0.25 Acetic Acid <100,     Acetophenone <2.5, Ammonium Hydroxide <100, Benzaldehyde <0.25,     Benzoin Resinoid <12.5, Benzyl Alcohol <100, Bergamot Oil <2.5,     Bornyl Acetate <0.25 Butyric Acid <0.25, Cardamon Seed Oil <0.25,     Carob Bean Extract <100, Celery Seed Oil <0.25, Chamomile Flower Oil     Hungarian <1.25, Chamomile Flower Oil Roman <1.25, Cinnamic Aldehyde     <12.5, Cinnamic Alcohol <0.25, Citral <0.25, Citric Acid <0.25, D,L     Citronellal <0.25, Clary Sage Oil <0.25, Cocoa and Cocoa extracts     <100, Coffee Extract <12.5, Cognac oil Green <0.25, Coriander Oil     <1.25, Davana Oil <0.25, Delta Decalactone <0.25, Gamma Decalactone     <0.25, Decanoic Acid <0.25, Diacetyl <0.25, Diammonium Phosphate     <100, 2,3-Dimethyl Pyrazine <0.25, Dill Oil <0.25, 2,5 Dimethyl     Pyrazine <0.25, Ethyl Acetate <12.5, Ethyl Hexanoate <12.5, Ethyl     Iso Valerate <0.25, Ethyl Lactate <0.25, Ethyl Maltol <0.25, Ethyl     Octanoate <0.25, Ethyl Phenylacetate <0.25, Ethyl Propionate <1.25,     Ethyl Vanillin <2.5, 5-Ethyl-3-Hydroxy-4-Methyl-2(5H)-Furanone     <0.25, Fenugreek Extract <2.5, Geraniol <0.25, Geranium Rose Oil     <0.25, Glycerine <100, 2-Heptanone <1.25, Hexanoic Acid <0.25, Hexyl     Acetate <0.25, 4-(Para-Hydroxyphenyl)-2-butanone <0.25, Immortelle     Extract <0.25, Alpha Ionone <0.25, Isoamyl Acetate <0.25, Isoamyl     Butyrate <0.25, Isoamyl Formate <0.25, Isoamyl Hexanoate <0.25,     Isoamyl Isovalerate <0.25, Isoamyl Phenyl Acetate <0.25, Iso Butric     Acid <1.25, Isovaleric Acid <0.25, Licorice Extract <100, Lime Oil     <1.25, Linalool <0.25, Lovage Extract <100, Maltol <12.5, Mate     Absolute <2.5, L-Menthol <100, 2-Mercapto Methyl Pyrazine <0.25,     Para-Methoxy Benzaldehyde <2.5, Methyl Isovalerate <0.25,     4-Methoxyacetphenone <1.25, 3-Methylbutyraldehyde <12.5, 2-Methyl     Butyric Acid <0.25, Methyl Cyclopentenelone <12.5, Mimosa Absolute     <0.25, Mountain Maple Extract <100, Gamma Nonalactone <0.25, Oakmoss     Absolute <2.5, Gamma Octalactone <0.25, Opoponox Oil <1.25, Orange     Oil <12.5, Orris Root Extract <12.5, Peppermint Oil <100,     Phenylethyl Alcohol <0.25, Phenylethyl Phenylacetate <12.5, Phenyl     Acetic Acid <0.25, Heliotropine <1.25, Vanitrope <0.25, Propylene     Glycol <100, Rhodinol <0.25, Rose Oil Otto Bulgarian <0.25, Rum     <100, Non-Alcoholic Rum <0.25, Sandalwood Oil <1.25, Scarolide <2.5,     Styrax Resin <0.25, High Fructose Corn Syrup 42% Solids <100, Invert     Sugar Syrup <100, Sucrose <100, Tangerine Oil <1.25, Alpha Terpineol     <1.25, 2,3,5,6 Tetramethylpyrazine <0.25, Para Tolyl Aldehyde <0.25,     4-(2,6,6-Trimethyl Cyclohex-1-enyl) but-2-en-one <0.25,     2,3,5-Trimethylpyrazine <0.25, Gamma Undecalactone <0.25, Valerian     Root Extract <100, Vanilla Bean Extract <2.5, Vanillin <25) (Chr.     Hansen) (18.18% W/W wet basis, 40.00% load dry basis). -   ii) Microcrystalline cellulose (Avicel PH101) (FMC Corp.)(45.45% W/W     wet basis, 60.00% load dry basis). -   iii) Deionized water (36.36% W/W wet basis).

The process comprises the steps used above in Examples 2-4. The resulting spheres can be introduced into a cigarette rod as described in Example 4 and flavor delivery evaluated.

This loading was optimal for a partially hydrophylic compound.

EXAMPLE 6

Described below is a process to deliver higher flavor load post rod filler in a cavity beneath the filter. This flavor contains high essential oil levels and the formula is optimized accordingly. Cellulose can be expected to swell, discharging flavor into entrained air flow.

Materials:

-   i) Tobacco Type flavor (composed of FEMA GRAS materials, the flavor     can be a mix consisting of the following at the limits not to exceed     the described maximum all described in percentage of the overall     flavoring preparation: Acetanisole <0.5, Acetic Acid <100,     Acetophenone <2.5, Ammonium Hydroxide <100, Benzaldehyde <0.5,     Benzoin Resinoid <25, Benzyl Alcohol <100, Bergamot Oil <0.5, Bornyl     Acetate <0.5, Butyric Acid <0.5, Cardamon Seed Oil <0.5, Carob Bean     Extract <100, Celery Seed Oil <0.5, Chamomile Flower Oil Hungarian     <2.5, Chamomile Flower Oil Roman <2.5, Cinnamic Aldehyde <25,     Cinnamic Alcohol <0.5, Citral <0.5, Citric Acid <0.5, D,L     Citronellal <0.5, Clary Sage Oil <2.5, Cocoa and Cocoa extracts     <100, Coffee Extract <25, Cognac oil Green <0.5, Coriander Oil <2.5,     Davana Oil <0.5, Delta Decalactone <0.5, Gamma Decalactone <0.5,     Decanoic Acid <0.5, Diacetyl <0.5, Diammonium Phosphate <100,     2,3-Dimethyl Pyrazine <0.5, Dill Oil <0.5, 2,5 Dimethyl Pyrazine     <0.5, Ethyl Acetate <25, Ethyl Hexanoate <25, Ethyl Iso Valerate     <0.5, Ethyl Lactate <0.5, Ethyl Maltol <0.5, Ethyl Octanoate <0.5,     Ethyl Phenylacetate <0.5, Ethyl Propionate <2.5, Ethyl Vanillin <5,     5-Ethyl-3-Hydroxy-4-Methyl-2(5H)-Furanone <0.5, Fenugreek Extract     <5, Geraniol <0.5, Geranium Rose Oil <0.5, Glycerine <100,     2-Heptanone <2.5, Hexanoic Acid <0.5, Hexyl Acetate <0.5,     4-(Para-Hydroxyphenyl)-2-butanone <0.5, Immortelle Extract <0.5,     Alpha Ionone <0.5, Isoamyl Acetate <0.5, Isoamyl Butyrate <0.5,     Isoamyl Formate <0.5, Isoamyl Hexanoate <0.5, Isoamyl Isovalerate     <0.5, Isoamyl Phenyl Acetate <0.5, Iso Butric Acid <2.5, Isovaleric     Acid <0.5, Licorice Extract <100, Lime Oil <2.5, Linalool <0.5,     Lovage Extract <50, Maltol <25, Mate Absolute <2.5, L-Menthol <100,     2-Mercapto Methyl Pyrazine <0.5, Para-Methoxy Benzaldehyde <5,     Methyl Isovalerate <1, 4-Methoxyacetphenone <2.5,     3-Methylbutyraldehyde <25, 2-Methyl Butyric Acid <0.5, Methyl     Cyclopentenelone <25, Mimosa Absolute <0.5, Mountain Maple Extract     <100, Gamma Nonalactone <0.5, Oakmoss Absolute <2.5, Gamma     Octalactone <0.5, Opoponox Oil <2.5, Orange Oil <25, Orris Root     Extract <25, Peppermint Oil <100, Phenylethyl Alcohol <0.5,     Phenylethyl Phenylacetate <25, Phenyl Acetic Acid <2.5, Heliotropine     <2.5 Vanitrope <0.5, Propylene Glycol <100, Rhodinol <0.5, Rose Oil     Otto Bulgarian <0.5, Rum <100, Non-Alcoholic Rum <0.5, Sandalwood     Oil <2.5, Scarolide <5, Styrax Resin <0.5, High Fructose Corn Syrup     42% Solids <100, Invert Sugar Syrup <100, Sucrose <100, Tangerine     Oil <2.5, Alpha Terpineol <2.5,-2,3,5,6 Tetramethylpyrazine <0.5,     Para Tolyl Aldehyde <0.5, 4-(2,6,6-Trimethyl Cyclohex-1-enyl)     but-2-en-one <0.5, 2,3,5-Trimethylpyrazine <0.5, Gamma Undecalactone     <0.5, Valerian Root Extract <100, Vanilla Bean Extract <5, Vanillin     <50) (Chr. Hansen) (9.76% W/W wet basis, 20.00 load dry basis). -   ii) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (48.78%     W/W wet basis, 80.00 load dry basis). -   iii) Deionized water (41.46% W/W wet basis).

The process comprises the following steps:

-   A) add Avicel and flavor to a planetary mixer; -   B) blend until visually uniform; -   C) add deionized water while mixing until visually uniform; -   D) extrude in a coaxial jacketed dome extruder to the     specifications: 0.7 mm stainless steel dieface at an auger speed of     45 rpm inserting 10 shims at the dome contact point; -   E) collect damp extrudate rods and deposit into a     Maumerizing/Spheronizing centrifugal unit—parameters are: 2.0 mm     disk plate at a speed of 800 rpm for a resonance time of 5 minutes;     and -   F) dry in Glatt Fluid Bed Dryer (<90° C.) target moisture is <20%.

The resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.10 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade. The cigarette can be lit in a conventional manner and flavor delivery evaluated.

EXAMPLE 7

Described below is a process to deliver highest menthol load post rod filler in a cavity beneath the filter. Menthol is not completely soluble and will polymerize on the surface of the spheres, not embedding completely within the matrix. This is optimum loading for menthol delivery. As noted above, cellulose will swell, discharging menthol into entrained air aerosol air flow.

Materials:

-   i) Menthol solution (40% Laevo Menthol Crystals, 30% glycerin, 30%     propylene glycol) (Chr. Hansen) (20.00% W/W wet basis, 28.57% load     dry basis). -   ii) Activated charcoal (American Norit Co.) (10.00% W/W wet basis,     14.29% load dry basis). -   iii) Diatomaceous earth (Silica) (Seegott Inc.) (5.00% W/W wet     basis, 7.14% load dry basis). -   iv) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (35.00%     W/W wet basis, 50.00). -   v) Deionized water (30.00% W/W wet basis).

The process comprises the following steps:

-   A) preblend Avicel, activated charcoal and diatomaceous earth in a     V-Blender until uniform; A1) add flavor to the above mixture in a     planetary mixer, while mixing; -   B) blend until visually uniform; -   C) add deionized water while mixing until visually uniform; -   D) extrude in a coaxial jacketed dome extruder to the     specifications: 0.5 mm stainless steel dieface at an auger speed of     45 rpm inserting 10 shims at the dome contact point; -   E) collect damp extrudate rods and deposit into a     Maumerizing/Spheronizing centrifugal unit—parameters are: 2.0 mm     disk plate at a speed of 1000 rpm for a resonance time of 3 minutes;     and -   F) dry in Glatt Fluid Bed Dryer (<90° C.) target moisture is <20%.

The resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.10 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade. The cigarette can be lit in a conventional manner and flavor delivery evaluated.

EXAMPLE 8

Described below is a process to deliver highest menthol load post rod filler in a cavity beneath the filter. Menthol is not completely soluble and will polymerize on the surface of the spheres, not embedding completely within the matrix. This is optimum loading for menthol delivery. Theoretically, cellulose will swell, discharging menthol into entrained air aerosol air flow. After observation of spheres upon storage, some polymerizaton occurred, indicating further optimization of the level. β-cyclodextrin was added to the matrix for covalent bonding of menthol.

Materials:

-   i) Solubilized menthol solution (40% Laevo Menthol Crystals, 30%     glycerin, 30% propylene glycol) (Chr. Hansen) (13.64% W/W wet basis,     23.08% load dry basis). -   ii) Beta cyclodextrin (Cerestar) (9.09% W/W wet basis, 15.38% load     dry basis). -   iii) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (36.36%     W/W wet basis, 61.54% load dry basis). -   iv) Deionized water (40.91% W/W wet basis).

The process comprises the following steps:

-   A) mix Avicel and cyclodextrin in a V-Blender until visually     uniform; -   B) add menthol solution and blend until visually uniform; -   C) add deionized water while mixing until visually uniform; -   D) extrude in a coaxial jacketed dome extruder to the     specifications: 0.5 mm stainless steel dieface at an auger speed of     45 rpm inserting 10 shims at the dome contact point; -   E) collect damp extrudate rods and deposit into a     Maumerizing/Spheronizing centrifugal unit—parameters are: 2.0 mm     disk plate at a speed of 1000 rpm for a resonance time of 2 minutes;     and -   F) dry in Glatt Fluid Bed Dryer (<90° C.) target moisture is <20%.

The resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.10 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade. The cigarette can be lit in a conventional manner and flavor delivery evaluated.

EXAMPLE 9

Described below is a process to deliver high flavor load post rod filler in a cavity beneath the filter. This flavor contains both flavor with menthol and the formula is optimized accordingly. Again, theoretically, cellulose will swell discharging flavor into entrained air flow.

Materials:

-   i) Tobacco Type flavor (composed of FEMA GRAS materials, the flavor     can be a mix consisting of the following at the limits not to exceed     the described maximum all described in percentage of the overall     flavoring preparation: Acetanisole <0.5, Acetic Acid <100,     Acetophenone <2.5, Ammonium Hydroxide <100, Benzaldehyde <0.5,     Benzoin Resinoid <25, Benzyl Alcohol <100, Bergamot Oil <0.5, Bornyl     Acetate <0.5, Butyric Acid <0.5, Cardamon Seed Oil <0.5, Carob Bean     Extract <100, Celery Seed Oil <0.5, Chamomile Flower Oil Hungarian     <2.5, Chamomile Flower Oil Roman <2.5, Cinnamic Aldehyde <25,     Cinnamic Alcohol <0.5, Citral <0.5, Citric Acid <0.5, D,L     Citronellal <0.5, Clary Sage Oil <2.5, Cocoa and Cocoa extracts     <100, Coffee Extract <25, Cognac oil Green <0.5, Coriander Oil <2.5,     Davana Oil <0.5, Delta Decalactone <0.5, Gamma Decalactone <0.5,     Decanoic Acid <0.5, Diacetyl <0.5, Diammonium Phosphate <100,     2,3-Dimethyl Pyrazine <0.5, Dill Oil <0.5, 2,5 Dimethyl Pyrazine     <0.5, Ethyl Acetate <25, Ethyl Hexanoate <25, Ethyl Iso Valerate     <0.5, Ethyl Lactate <0.5, Ethyl Maltol <0.5, Ethyl Octanoate <0.5,     Ethyl Phenylacetate <0.5, Ethyl Propionate <2.5, Ethyl Vanillin <5,     5-Ethyl-3-Hydroxy-4-Methyl-2(5H)-Furanone <0.5, Fenugreek Extract     <5, Geraniol <0.5, Geranium Rose Oil <0.5, Glycerine <100,     2-Heptanone <2.5, Hexanoic Acid <0.5, Hexyl Acetate <0.5,     4-(Para-Hydroxyphenyl)-2-butanone <0.5, Immortelle Extract <0.5,     Alpha Ionone <0.5, Isoamyl Acetate <0.5, Isoamyl Butyrate <0.5,     Isoamyl Formate <0.5, Isoamyl Hexanoate <0.5, Isoamyl Isovalerate     <0.5, Isoamyl Phenyl Acetate <0.5, Iso Butric Acid <2.5, Isovaleric     Acid <0.5, Licorice Extract <100, Lime Oil <2.5, Linalool <0.5,     Lovage Extract <50, Maltol <25, Mate Absolute <2.5, L-Menthol <100,     2-Mercapto Methyl Pyrazine <0.5, Para-Methoxy Benzaldehyde <5,     Methyl Isovalerate <1, 4-Methoxyacetphenone <2.5,     3-Methylbutyraldehyde <25, 2-Methyl Butyric Acid <0.5, Methyl     Cyclopentenelone <25, Mimosa Absolute <0.5, Mountain Maple Extract     <100, Gamma Nonalactone <0.5, Oakmoss Absolute <2.5, Gamma     Octalactone <0.5, Opoponox Oil <2.5, Orange Oil <25, Orris Root     Extract <25, Peppermint Oil <100, Phenylethyl Alcohol <0.5,     Phenylethyl Phenylacetate <25, Phenyl Acetic Acid <2.5, Heliotropine     <2.5 Vanitrope <0.5, Propylene Glycol <100, Rhodinol <0.5, Rose Oil     Otto Bulgarian <0.5, Rum <100, Non-Alcoholic Rum <0.5, Sandalwood     Oil <2.5, Scarolide <5, Styrax Resin <0.5, High Fructose Corn Syrup     42% Solids <100, Invert Sugar Syrup <100, Sucrose <100, Tangerine     Oil <2.5, Alpha Terpineol <2.5, 2,3,5,6 Tetramethylpyrazine <0.5,     Para Tolyl Aldehyde <0.5, 4-(2,6,6-Trimethyl Cyclohex-1-enyl)     but-2-en-one <0.5, 2,3,5-Trimethylpyrazine <0.5, Gamma Undecalactone     <0.5, Valerian Root Extract <100, Vanilla Bean Extract <5, Vanillin     <50) (Chr. Hansen) (10.00% W/W wet basis, 16.67% load dry basis). -   ii) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (50.00%     W/W wet basis, 83.33% load dry basis). -   iii) Deionized water (40.00% W/W wet basis).

The process comprises the following steps:

-   A) add Avicel and flavor to a planetary mixer; -   B) blend until visually uniform; -   C) add deionized water while mixing until visually uniform; -   D) extrude in a coaxial jacketed dome extruder to the     specifications: 0.7 mm stainless steel dieface at an auger speed of     45 rpm inserting 10 shims at the dome contact point; -   E) collect damp extrudate rods and deposit into a     Maumerizing/Spheronizing centrifugal unit—parameters are: 2.0 mm     disk plate at a speed of 1000 rpm for a resonance time of 3 minutes;     and -   F) dry in Glatt Fluid Bed Dryer (<90° C.) target moisture is <20%.

The resulting spheres can be introduced into a cigarette rod in the manner described in Example 8 and flavor delivery evaluated.

EXAMPLE 10

Described below is a process to deliver highest oil soluble flavor load post rod filler in a cavity beneath the filter. Oil soluble flavors will only partially embedded (fully bind) within the matrix and can form oily deposits on the surface of the sphere releasing flavor upon storage. This is optimum loading for oil based flavor delivery. As pointed out above, theoretically, cellulose will swell discharging menthol into entrained air aerosol air flow. After observation of spheres upon storage, some polymerization occurs, indicating that hydrophobic complexation is needed to bind the flavor to the matrix. β-cyclodextrin is added to the matrix for covalent bonding of oil soluble raw materials.

Materials:

-   i) Tobacco Type flavor (composed of FEMA GRAS materials, the flavor     can be a mix consisting of the following at the limits not to exceed     the described maximum all described in percentage of the overall     flavoring preparation: Acetanisole <0.25 Acetic Acid <100,     Acetophenone <2.5, Ammonium Hydroxide <100, Benzaldehyde <0.25,     Benzoin Resinoid <12.5, Benzyl Alcohol <100, Bergamot Oil <2.5,     Bornyl Acetate <0.25 Butyric Acid <0.25, Cardamon Seed Oil <0.25,     Carob Bean Extract <100, Celery Seed Oil <0.25, Chamomile Flower Oil     Hungarian <1.25, Chamomile Flower Oil Roman <1.25, Cinnamic Aldehyde     <12.5, Cinnamic Alcohol <0.25, Citral <0.25, Citric Acid <0.25, D,L     Citronellal <0.25, Clary Sage Oil <0.25, Cocoa and Cocoa extracts     <100, Coffee Extract <12.5, Cognac oil Green <0.25, Coriander Oil     <1.25, Davana Oil <0.25, Delta Decalactone <0.25, Gamma Decalactone     <0.25, Decanoic Acid <0.25, Diacetyl <0.25, Diammonium Phosphate     <100, 2,3-Dimethyl Pyrazine <0.25, Dill Oil <0.25, 2,5 Dimethyl     Pyrazine <0.25, Ethyl Acetate <12.5, Ethyl Hexanoate <12.5, Ethyl     Iso Valerate <0.25, Ethyl Lactate <0.25, Ethyl Maltol <0.25, Ethyl     Octanoate <0.25, Ethyl Phenylacetate <0.25, Ethyl Propionate <1.25,     Ethyl Vanillin <2.5, 5-Ethyl-3-Hydroxy-4-Methyl-2(5H)-Furanone     <0.25, Fenugreek Extract <2.5, Geraniol <0.25, Geranium Rose Oil     <0.25, Glycerine <100, 2-Heptanone <1.25, Hexanoic Acid <0.25, Hexyl     Acetate <0.25, 4-(Para-Hydroxyphenyl)-2-butanone <0.25, Immortelle     Extract <0.25, Alpha Ionone <0.25, Isoamyl Acetate <0.25, Isoamyl     Butyrate <0.25, Isoamyl Formate <0.25, Isoamyl Hexanoate <0.25,     Isoamyl Isovalerate <0.25, Isoamyl Phenyl Acetate <0.25, Iso Butric     Acid <1.25, Isovaleric Acid <0.25, Licorice Extract <100, Lime Oil     <1.25, Linalool <0.25, Lovage Extract <100, Maltol <12.5, Mate     Absolute <2.5, L-Menthol <100, 2-Mercapto Methyl Pyrazine <0.25,     Para-Methoxy Benzaldehyde <2.5, Methyl Isovalerate <0.25,     4-Methoxyacetphenone <1.25, 3-Methylbutyraldehyde <12.5, 2-Methyl     Butyric Acid <0.25, Methyl Cyclopentenelone <12.5, Mimosa Absolute     <0.25, Mountain Maple Extract <100, Gamma Nonalactone <0.25, Oakmoss     Absolute <2.5, Gamma Octalactone <0.25, Opoponox Oil <1.25, Orange     Oil <12.5, Orris Root Extract <12.5, Peppermint Oil <100,     Phenylethyl Alcohol <0.25, Phenylethyl Phenylacetate <12.5, Phenyl     Acetic Acid <0.25, Heliotropine <1.25, Vanitrope <0.25, Propylene     Glycol <100, Rhodinol <0.25, Rose Oil Otto Bulgarian <0.25, Rum     <100, Non-Alcoholic Rum <0.25, Sandalwood Oil <1.25, Scarolide <2.5,     Styrax Resin <0.25, High Fructose Corn Syrup 42% Solids <100, Invert     Sugar Syrup <100, Sucrose <100, Tangerine Oil <1.25, Alpha Terpineol     <1.25, 2,3,5,6 Tetramethylpyrazine <0.25, Para Tolyl Aldehyde <0.25,     4-(2,6,6-Trimethyl Cyclohex-1-enyl) but-2-en-one <0.25,     2,3,5-Trimethylpyrazine <0.25, Gamma Undecalactone <0.25, Valerian     Root Extract <100, Vanilla Bean Extract <2.5, Vanillin <25) (Chr.     Hansen) (19.05% W/W wet basis, 28.57% load dry basis). -   ii) Beta cyclodextrin (Cerestar) (9.52% W/W wet basis, 14.28% load     dry basis). -   iii) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (38.10%     W/W wet basis, 57.15% load dry basis). -   iv) Deionized water (33.33% W/W wet basis).

The process comprises the following steps:

-   A) mix Avicel and cyclodextrin in a V-Blender until visually     uniform; -   B) add flavor and blend until visually uniform; -   C) add deionized water while mixing until visually uniform; -   D) extrude in a coaxial jacketed dome extruder to the     specifications: 0.5 mm stainless steel dieface at an auger speed of     45 rpm inserting 10 shims at the dome contact point; -   E) collect damp extrudate rods and deposit into a     Maumerizing/Spheronizing centrifugal unit—parameters are: 2.0 mm     disk plate at a speed of 800 rpm for a resonance time of 3 minutes;     and -   F) dry in Glatt Fluid Bed Dryer (<90° C.) target moisture is <20%.

The resulting spheres can be introduced into a cigarette rod and flavor delivery evaluated in the manner described in Example 8.

EXAMPLE 11

Described below is a process to deliver placebo spheres for machine filling capabilities. No flavor is contained in this product. It is a space holder within the cavity.

Materials (Placebo):

-   i) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (50.00% W/W     wet basis, 100.00% load dry basis). -   ii) Deionized water (50.00% W/W wet basis).

The process comprises the following steps:

-   A) add Avicel and deionized water in a planetary mixer; -   B) blend until visually uniform; -   C) extrude in a coaxial jacketed dome extruder to the     specifications: 0.7 mm stainless steel dieface at an auger speed of     45 rpm inserting 10 shims at the dome contact point; -   D) collect damp extrudate rods and deposit into a     Maumerizing/Spheronizing centrifugal unit—parameters are: 2.0 mm     disk plate at a speed of 800 rpm for a resonance time of 5 minutes;     and -   E) dry in Glatt Fluid Bed Dryer (<90° C.) target moisture is <20%.

The resulting spheres can be introduced into a cigarette rod and flavor delivery evaluated in the manner described in Example 8.

EXAMPLE 12

Described below is a process to embed glycerin within spheres to provide a vapor aerosol effect. These are to be used in conjunction with flavor spheres to provide volatile aerosol to deliver more flavor in the steam entrainment.

Materials (Glycerin Aerosol):

-   i) Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (48.97% W/W     wet basis, 70.00% load dry basis). -   ii) Glycerin (Ashland Chemical) (21.06% W/W wet basis, 30.00% load     dry basis). -   iii) Deionized water (29.97% W/W wet basis).

The process comprises the following steps:

-   A) add Avicel and Glycerin to a planetary mixer; -   B) blend until visually uniform; -   C) add deionized water while mixing until visually uniform; -   D) extrude in a coaxial jacketed dome extruder to the     specifications: 0.7 mm stainless steel dieface at an auger speed of     45 rpm inserting 7 shims at the dome contact point; -   E) collect damp extrudate rods and deposit into a     Maumerizing/Spheronizing centrifugal unit—parameters are: 2.0 mm     disk plate at a speed of 1000 rpm, 60° C. jacket, for a resonance     time of 2 minutes; and -   F) dry in a kugelcoater 65° C. 20 minutes, 150m³ /hr air volume.

The resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.05-0.10 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade. The cigarette can be lit in a conventional manner and flavor delivery evaluated.

All of the formulations above can be polymer coated concurrent with drying or post dried. The coating can contain an additional 2-5% of flavoring. Referenced below is an example of coating preparation and application to the spheres.

EXAMPLE 13

Described below is a process to prepare coating and a method of coating the spheres.

Materials:

-   i) Dri-Klear-091 (fine granulation hydroxypropyl methyl cellulose)     (100.00% Solids) (Chr. Hansen) (10.00% W/W wet basis, 10.00% load     dry basis). -   ii) Deionized water (0% solids) (90.00% W/W wet basis).

The process comprises the following steps:

-   A) mix Dri-Clear (hydroxypropyl methyl cellulose (FMC) with water     until solution is formed; -   B) charge drier/coater with flavor spheres; -   C) spray (1) on a dry basis of hydroxypropyl methyl cellulose (HPMC)     2.5% wt (solid HPMC) of the total sphere batch on a dry weight basis     @ 100% efficiency. Spray rate of 18-20 gms/minute in a 65-80° C.     chamber, exhaust 48-49° C. Air Flow 100-110 CFM 40-42 PSI; and -   D) dry for 5 minutes or until exhaust reaches 60° C. Disconnect dust     collection, shut down and discharge unit, empty spheres, sift thru     28 mesh screen to qualify 0.7 mm size particles.

Application in cigarettes for stability study of uncoated spheres vs. coated spheres. The coated spheres have greater longer term stability than the uncoated spheres. 

1. A spherical particle comprising a matrix material and at least one flavoring agent absorbed therein.
 2. The particle of claim 1 wherein said matrix material is selected from the group consisting of cellulose, starch, gum, pectin and protein.
 3. The particle of claim 2 wherein said matrix material is microcrystalline cellulose.
 4. The particle of claim 1 wherein said particle further comprises at least one additive selected from the group consisting of activated carbon, diatomaceous earch, silica, silicates, α-cyclodextrin, β-cyclodextrin and γ-cyclodextrin.
 5. The particle of claim 1 wherein said flavoring agent is selected from the group consisting of menthol, vanillin, cocoa and licorice.
 6. The particle of claim 1 wherein said particle further comprises an agent that promotes aerosolization.
 7. The particle of claim 6 wherein said agent that promotes aerosolization is selected from the group consisting of glycerin, propylene glycol and triethylene glycol.
 8. The particle of claim 7 wherein the agent that promotes aerosolization is glycerin.
 9. The particle of claim 8 wherein said particle is about 10% to about 40% (w/w) glycerin.
 10. The particle of claim 1 wherein said particle further comprises a coating.
 11. The particle of claim 10 wherein said coating is hydroxylpropylmethyl cellulose or carboxymethyl cellulose.
 12. The particle of claim 1 wherein said particle is about 0.3 mm to about 10 mm in diameter.
 13. A spherical particle comprising a matrix material and an agent that promotes aerosolization absorbed therein.
 14. A method of preparing the particle of claim 1 comprising: (a) mixing a liquid comprising said flavoring agent and dry matrix material to form a dough-like paste; (b) feeding the dough-like paste resulting from step (a) into an extruder and extruding the dough-like paste into rods; (c) introducing the rods resulting from step (b) into a spheronizing unit so that said rods contact a spinning friction plate within said unit and are propelled against the inside wall of said unit by centrifugal force, whereby said rods are broken into smaller segments that, by centrifugal and gravitational forces, create a mechanically fluidized ring of particles of essentially uniform spherical shape; and (d) drying the particles resulting from step (c).
 15. The method of claim 14 wherein said method further comprises, after step (d), thin film coating the particles resulting from step (d).
 16. The method of claim 15 wherein said extruder is a low-pressure extruder.
 17. An intermediate product comprising a dough-like paste comprising a mixture of a matrix material that absorbs fluid 2-5 times its weight in fluid and a liquid comprising a flavoring agent.
 18. A smokable article comprising at least one particle of claim 1, wherein said particle is positioned in said article such that said flavoring agent is released from said matrix material through non-pyrolysis steam entrainment.
 19. The article of claim 18 wherein said article is a cigarette.
 20. The article of claim 19 wherein said cigarette comprises a tobacco rod filler and a filter and said at least one particle is located between said filler and said filter. 